tert-Butanol → 4-chloro-5,8-difluoro-N-(4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)phthalazin-1-amine

HRID 911137ノート

反応式

HRID 911137 の反応式
[NH2:1][C:2]1[CH:22]=[CH:21][C:5]([O:6][C:7]2[C:12]([C:13]3[CH:18]=[CH:17][N:16]=[C:15]([NH:19][CH3:20])[N:14]=3)=[CH:11][CH:10]=[CH:9][N:8]=2)=[CH:4][CH:3]=1.[Cl:23][C:24]1[C:33]2[C:28](=[C:29]([F:35])[CH:30]=[CH:31][C:32]=2[F:34])[C:27](Cl)=[N:26][N:25]=1.CC(O)(C)C>C(OCC)C>[Cl:23][C:24]1[C:33]2[C:28](=[C:29]([F:35])[CH:30]=[CH:31][C:32]=2[F:34])[C:27]([NH:1][C:2]2[CH:22]=[CH:21][C:5]([O:6][C:7]3[C:12]([C:13]4[CH:18]=[CH:17][N:16]=[C:15]([NH:19][CH3:20])[N:14]=4)=[CH:11][CH:10]=[CH:9][N:8]=3)=[CH:4][CH:3]=2)=[N:26][N:25]=1

参加物

5

反応物 3

HCID 6386tert-ButanolHCID 183618711,4-Dichloro-5,8-difluorophthalazineHCID 469295414-(2-(4-aminophenoxy)pyridin-3-yl)-N-methylpyrimidin-2-amine

生成物 1

HCID 577562244-chloro-5,8-difluoro-N-(4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)phthalazin-1-amine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
100 °C

実験手順

To 4-(2-(4-aminophenoxy)pyridin-3-yl)-N-methylpyrimidin-2-amine (0.100 g, 0.34 mmol) and 1,4-dichloro-5,8-difluorophthalazine (0.096 g, 0.41 mmol) was added tBuOH (1.0 mL). The resulting mixture was heated to 100° C. in a sealed tube for 45 min. The reaction was diluted with diethyl ether and the resulting solids were filtered and triturated with EtOAc. The solids were dried to yield 4-chloro-5,8-difluoro-N-(4-(3-(2-(methylamino)pyrimidin-4-yl)pyridin-2-yloxy)phenyl)phthalazin-1-amine as a dark gray solid. MS m/z=492 [M+H]+. Calc'd for C24H16ClF2N7O: 491.89.

後処理

  1. filtrationthe resulting solids were filtered
  2. customtriturated with EtOAc
  3. customThe solids were dried

出典と根拠

ORDレコード
ord-c3a1ef4828ca4a80b75a72bd1eecfb0c
出典データセット
uspto-grants-2011_09
特許番号
US08022221B2

反応ノート

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